高钙碳酸盐岩样品中微量钛ICP-MS测试方法OA北大核心CSTPCD
Determination of Trace Ti in High Calcium Carbonate Rocks by ICP-MS
硅酸岩中的主量元素钛(Ti)在碳酸盐岩中含量一般低于3.5mg/g,其中绝大部分低于1mg/g,目前常用于硅酸岩中Ti含量(通常大于0.1%)测试的X射线荧光光谱法已无法满足碳酸盐岩中微量Ti的准确测试要求.本文尝试用电感耦合等离子体质谱测试碳酸盐岩中的Ti含量,讨论分析了 Ti的5个测试同位素(46Ti、47 Ti、48 Ti、49 Ti、50 Ti)在碳酸盐岩基体中的受干扰情况,确定了适合的测试同位素48Ti,从而提出碳酸盐岩中微量Ti的ICP-MS测试方法.按照该方法测试并校正5个国家一级标准物质中Ti浓度,测定值与标准值相符,相对标准偏差(RSD,n=10)小于7.3%.在同一实验条件下,测试未知碳酸盐岩样品溶液Ti浓度并加以校正,与国家标准方法二安替比林甲烷光度法及电感耦合等离子体发射光谱法(ICP-OES)测定结果进行方法比对,与两者的相对标准偏差均小于允许限.方法加标回收率为83%~107%.该方法适用于CaO含量范围在31%~56%,Ti含量范围在14~3346μg/g的碳酸盐岩样品的测试,为高钙高镁碳酸盐岩中微量Ti的测试提供了方法参考.
The content of Ti in carbonate rocks is generally lower than 3.5mg/g,and most of it is below 1mg/g.X-ray fluorescence spectrometry(XRF),which is commonly used to measure Ti content in silicic rocks(usually more than 0.1%),cannot meet the requirements of accurate measurement of trace Ti in carbonate rocks.This paper reports on the attempts to test Ti in carbonate rock by inductively coupled plasma-mass spectrometry(ICP-MS),discusses and analyzes the interference of 5 test isotopes of Ti(46Ti,47Ti,48Ti,49Ti,50Ti)in carbonate solution matrix,and determines the suitable test isotope 48Ti.Then the ICP-MS method for the determination of trace Ti in carbonate rock is proposed.According to the method,the concentration of Ti in 5 first-class national standard materials was tested and corrected.The measured values were consistent with the certified values,and the relative standard deviation(RSD,n=10)was less than 7.3%.The concentration of Ti in the unknown carbonate sample solution was measured and corrected under the same experimental conditions,and this method was compared with the national standard method of diantipyrine methane spectrophotometry and inductively coupled plasma-optical emission spectrometry(ICP-OES)method,and the relative standard deviation with these two methods were less than the allowable limit.The recoveries were 83%-107%.This method is suitable for the determination of carbonate samples with 31%-56%CaO and 14-3346pg/g Ti,and provides a reference for the determination of trace Ti in carbonate rocks with high calcium and magnesium.
陈菲菲;金斌;杨梦娜;陈瑜;冉敬;徐国栋
中国地质调查局成都地质调查中心,四川成都 610081
地质学
碳酸盐岩电感耦合等离子体质谱法Ti同位素选择
carbonate rocksinductively coupled plasma-mass spectrometryTiisotope selection
《岩矿测试》 2024 (004)
558-567 / 10
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